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At least 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Insights into Preceramic Polymer-Based Additive Manufacturing Inks via Rheological and Scattering Studies of Preceramic Polymer-Grafted Nanoparticles Suspended in Polycarbosilane

Preceramic polymers (PCPs) offer advantages in producing ceramics due to their processability and ability to tailor the final chemistry of the produced material. However, challenges such as volumetric shrinkage and mass loss during pyrolysis often result in polymer-derived ceramics containing pores and cracks. PCP-grafted ceramic nanoparticles (PCPGNPs) have been proposed and studied as a route to mitigate the shrinkage issues associated with neat PCPs. Prior studies on PCPGNPs have principally focused on the synthesis and characterization of neat materials. Dispersing PCPGNPs in commercial preceramic polymer is another attractive, but underexplored, route to control the rheological and char yield properties of PCP systems. In this work, a systematic rheological study of commercial PCP (SMP-877) and PCPGNP (silica with poly(1,1-dimethylpropylsilane) corona) mixtures was executed to develop design rules for the processing of such systems. A rheological study demonstrated the effect of increasing particle concentration on network formation with percolation occurring between 50 and 60 wt %. Samples above the percolation threshold exhibited higher viscosities and rapid shear thinning thus demonstrating their direct-write printability. X-ray photon correlation spectroscopy (XPCS) corroborated the rheology and showed two diffusive modes when the material was above percolation. Mixtures of PCPGNPs and SMP-877 had synergistically higher char yields upon thermal treatment and pyrolysis. XPCS and rheological measurements during thermal treatment identified thermal jamming of the polymer grafts as a key factor in improving the char yield. In conclusion, with the insights gained here, we expect these mixed systems to provide attractive feedstocks for polymer-derived ceramics, with proof-of-principal application as feedstocks for direct ink write (DIW) additive manufacturing.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Indirect additive manufacturing process for producing SiC—B4C—Si composites

A method for indirect additive manufacturing of an object constructed of boron carbide, silicon carbide, and free silicon, comprising: (i) producing a porous preform constructed of boron carbide and silicon carbide by an indirect ceramic additive manufacturing (ICAM) process in which particles of a powder mixture become bonded together with an organic binder, wherein the powder mixture comprises: a) boron carbide particles, and b) silicon carbide particles, wherein at least 80 vol % of the silicon carbide particles are larger than the boron carbide particles; and wherein the boron carbide and silicon carbide particles are each included in an amount of 40-60 wt. % of the powder mixture, provided that the foregoing amounts sum to at least 95 wt. %; (ii) subjecting the porous preform to a temperature of 500-900° C. to volatilize the organic binder; and (iii) infiltrating molten silicon into pores of the porous preform to produce the object.

Cramer, Corson L.↗
DOE OSTI2016

Near room temperature magnetodielectric consequence in (Li, Ti) doped NiO ceramic

In the quest for high-k dielectrics with decent magnetodielectric (MD) response, ball-milled processed (Li, Ti) doped NiO ceramics have been evaluated by various experimental techniques. Magnetic properties in these ceramics manifest with a pronounced anomaly appearing at ∼260 K, suggesting ferrimagnetic phase (related to cluster magnetism) and co-existence with a glassy-like antiferromagnetic phase at ∼7 K. Room temperature neutron diffraction pattern shows the existence of short-range magnetic correlations. In the magnetically ordered state below 250 K, the magnetic structure is found to be phase coexistence of G-type antiferromagnet and ferrimagnet. Impedance spectroscopy measurements over a wide temperature range can be perfectly described with appropriate microstructural model (internal barrier layer capacitor), based on domain and domain boundary relaxations, justifying the enhancement of the dielectric response. The low-temperature (T < 100 K) dielectric relaxation is polaronic in nature, associated with the charge ordering of a mixed valence states of Ti ions (co-existence of Ti{sup 3+} and Ti{sup 4+}). Finally, our investigations in external magnetic fields up to 15 T reveal the occurrence of negative MD effect near room temperature. This intriguing intrinsic feature has been understood by the mechanism of charge-hopping-mediated MD effects.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2024

UHT-CAMANCHE: Ultra-High Temperature Ceramic Additively Manufactured Compact Heat Exchangers

The conceptual basis for this project is the convergence of advanced ultra-high temperature ceramic materials and additive manufacturing technologies to produce compact ceramic heat exchangers with complex internal flow path geometries. Task areas were broadly divided into materials and manufacturing development, heat exchanger design, component testing, and techno-economic analysis. Technical challenges included the design and commissioning of new test facilities, improving feature resolution and deposition rate of ceramic additive manufacturing techniques, establishing process-structure-property relationships in additively manufactured ultra-high temperature ceramics, and assessing high temperature materials compatibility in CO 2 environments. The primary candidate material evaluated in this work is a composite comprising zirconium diboride (ZrB2) with 30 vol. % silicon carbide (SiC) which was selected based on its desirable combination of high temperature mechanical properties, high thermal and electrical conductivities, and oxidation resistance. High solids loaded ZrB2-SiC pastes suitable for extrusion-based additive manufacturing were developed for the first time as part of this work. Materials compatibility studies indicate this material oxidizes in CO 2 to form a protective borosilicate scale which transforms to pure silica above 1000°C. Parts made by additive manufacturing displayed enlarged grain sizes produced by pressureless sintering as compared to hot-press sintering. Increases in microstructural coarseness have outsized effect on oxidation performance up to 1400°C due to incomplete oxidation of coarse large diameter SiC particles resulting in lower amounts of silica that apparently inhibit protective scale formation. Additive manufacturing as a forming technique did not appear to significantly affect thermal conductivity, hardness, or elastic modulus, though flexural strength was reduced by half or more as compared to traditionally hot-pressed materials. This effect was attributed to the presence of strength-limiting flaws (ca. 40 microns in size) originating from extrudate inhomogeneities that could potentially be eliminated with further process improvements. Attempts to attain economies of scale for production of multi-kilowatt scale heat exchangers by ceramic additive manufacturing proved difficult. Lack of automation and a modest extrusion rate while retaining fine feature resolution made the overall process labor intensive and limited experimental throughput. A number of full-scale components were taken through post-process heat treatments including drying, binder burnout, and sintering; however, none survived without significant flaws or cracks. Therefore, no operational data from a newly installed heat exchanger test loop were able to be obtained during the performance period. Continued research and development is recommended to improve economic feasibility of ceramic additive manufacturing by standardizing the use of advanced sensors, artificial intelligence, and automation tools to reduce associated labor costs and accelerate production rates. The materials and manufacturing techniques demonstrated in this work are likely to find applications in defense and energy applications.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2014

Ceramic Waste Form Data Package

The purpose of this data package is to provide information about simulated crystalline waste forms that can be used to select an appropriate composition for a Cold Crucible Induction Melter (CCIM) proof of principle demonstration. Melt processing, viscosity, electrical conductivity, and thermal analysis information was collected to assess the ability of two potential candidate ceramic compositions to be processed in the Idaho National Laboratory (INL) CCIM and to guide processing parameters for the CCIM operation. Given uncertainties in the CCIM capabilities to reach certain temperatures throughout the system, one waste form designated 'Fe-MP' was designed towards enabling processing and another, designated 'CAF-5%TM-MP' was designed towards optimized microstructure. Melt processing studies confirmed both compositions could be poured from a crucible at 1600°C although the CAF-5%TM-MP composition froze before pouring was complete due to rapid crystallization (upon cooling). X-ray diffraction measurements confirmed the crystalline nature and phase assemblages of the compositions. The kinetics of melting and crystallization appeared to vary significantly between the compositions. Impedance spectroscopy results indicated the electrical conductivity is acceptable with respect to processing in the CCIM. The success of processing either ceramic composition will depend on the thermal profiles throughout the CCIM. In particular, the working temperature of the pour spout relative to the bulk melter which can approach 1700°C. The Fe-MP composition is recommended to demonstrate proof of principle for crystalline simulated waste forms considering the current configuration of INL's CCIM. If proposed modifications to the CCIM can maintain a nominal temperature of 1600°C throughout the melter, drain, and pour spout, then the CAF-5%TM-MP composition should be considered for a proof of principle demonstration.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Processing of crack-free high density polycrystalline LiTaO3 ceramics

Our work achieved high density (99.9%) polycrystalline LiTaO 3 . The keys to the high density without cracking were the use of LiF-assisted densification to maintain fine grain size as well as the presence of secondary lithium aluminate phases as grain growth inhibitors. The average grain size of the hot pressed polycrystalline LiTaO 3 is less than 5 μm, limiting residual stresses caused by the anisotropic thermal expansion. Dilatometry results clearly indicate liquid phase sintering via the added LiF sintering aid. Efficient liquid phase sintering allows densification during low temperature hot pressing. Electron microscopy confirmed the high-density microstructure. Furthermore, Rietveld analysis of neutron diffraction data revealed the presence of LiAlO 2 and LiAl 5 O 8 minority phases and negligible substitutional defect incorporation in LiTaO 3 .

36 MATERIALS SCIENCE↗
DOE OSTI2017

Commercialization of Ultra-Hard Ceramics for Cutting Tools Final Report CRADA No. TC0279.0

This was a collaborative effort between Lawrence Livermore National Security, LLC as manager and operator of Lawrence Livermore National Laboratory (LLNL) and Greenleaf Corporation (Greenleaf) to develop the technology for forming unique precursor nano-powders process that can be consolidated into ceramic products for industry. LLNL researchers have developed a solgel process for forming nano-ceramic powders. The nano powders are highly tailorable, allowing the explicit design of desired properties that lead to ultra hard materials with fine grain size. The present CRADA would allow the two parties to continue the development of the sol-gel process and the consolidation process in order to develop an industrially sound process for the manufacture of these ultra-hard materials.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Applying molecular dynamics simulations to the study of micro cold spray of yttria

Micro cold spray (MCS) is a novel manufacturing process with proven success depositing dense, thick films of technical ceramics without the need for elevated processing temperatures or chemical precursors. The process transforms a loose sub-micrometer powder into an adherent film with mechanical properties approaching that of the bulk material through a phenomenon known as room temperature impact consolidation. While this phenomenon has been demonstrated for a wide variety of ceramic materials and film substrates, yttria stands out as a material that is both well-characterized in experiments and of significant interest for industrial applications due to its excellent refractory properties. This dissertation seeks to investigate the fundamental mechanisms that enable room temperature impact consolidation by using molecular dynamics (MD) simulations of yttria particle impacts and characterizing the deformation behavior of the system.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Study of Ion Conductivity and Chain Dynamics in Polymer-Ceramic Composite Electrolytes

We fabricated polymer-ceramic composite consisting of polyethylene oxide, lithium trifluoromethanesulfonate, and a lithium-conducting glass ceramic from Ohara corporation. We examined the ion conductivity of the composite electrolyte with high volume fractions of Ohara ceramic (30% to 60%) using various processing methods. In this composition range, the composite conductivity was less affected by the volume fraction of the ceramic. Instead, it was strongly affected by processing methods. We found that the composite showed lower ion conductivity than the conductivity of PEO and the Ohara ceramic. A trilayer experiment using polymer electrolyte/Ohara ceramic plate/polymer electrolyte design revealed a very large interfacial resistance between the polymer electrolyte and Ohara ceramic. Quasi-elastic neutron scattering measurements were performed on the system to shed light on underpinnings of the origin of this large interfacial resistance.

Chen, Xi↗
DOE OSTI2020

Recipe for coating ceramic blades for ion trapping

The first batches of ion traps patterned and coated were processed per the standard 3-step clean, air fire, and metallization processes. The third or fourth lot using this process resulted in poorly adhering metallization. Up until this point, the standard process was used to metallize and pattern ceramic ion traps without fail. At about the 4th batch of parts something changed. After the 5th batch, the ceramic ion traps received generally came with some unknown contamination that does not come off in a standard 3-step clean (Lenium Vapor Degreaser, Acetone, IPA) and air fire (860C for 1 hour) for which this process removes the vast majority of all contamination for most ceramic metallization. This is highly unusual. Using HF + Boiling H 2 O 2 is extreme for cleaning the ceramic ion traps. The contamination was never identified and is stubborn to effectively clean. Standard as-fired ceramic should be very easy to clean as if s fired at temperatures greater than 1400°C and not much in terms of contamination should exist at these temperatures, so there must be an intermediate step/process which is imparting this contamination. It is likely a polishing compound or previous polishing contaminant, but also not easily visually distinguishable until after metallization. The halo marks observed on parts might be fingerprints (less likely) or potential polishing marks (more likely) as metallization typically doesn't cover/hide any damage or contamination, but rather quite clearly the opposite, it accentuates it. Blotchy appearances in the metallization usually indicated an adhesion issue. As a result of the fragility of the parts (yield loss due to handling) and difficulty in identifying the contamination during cleaning, we have taken a conservative approach of HF + H 2 O 2 cleaning for all batches after the contamination and adhesion issues were identified.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Scalable Solution-Processed Electrolyte Membranes with Optimized Microstructure for High-Performance Protonic Ceramic Electrochemical Cells

Proton-conducting electrochemical cells (PCECs) are promising for efficient hydrogen production, but achieving dense, uniform, thin electrolyte layers remains a key challenge, particularly for scalable fabrication. Here, we present a solution-processed deposition approach with a mechanistically optimized slurry for uniform electrolyte formation. By tailoring particle size distribution, solid loading, and solvent/additive balance, we regulated wetting behavior and evaporation kinetics of the electrolyte slurry to promote homogeneous electrolyte particle packing. These features facilitate tight grain boundary contact and early stage neck growth during sintering, eliminating residual porosity, and improving mechanical integrity. The resulting ∼15 μm thick electrolyte shows high density, strong electrode adhesion, and stable interfaces outperforming the previously reported spray-based fabricated electrolyte by about 31% at 600 °C in FC mode. Single cells deliver 0.962 W cm –2 at 600 °C in fuel cell mode and 1.31 A cm –2 at 1.3 V in electrolysis mode, maintaining robust performance over 100 h with negligible degradation (≤0.02% h –1 ) in each mode. Scale-up to 2.5 cm diameter substrates confirmed reproducible densification and geometric stability. This work demonstrates a cost-effective, scalable route where control over particle-fluid interactions and drying dynamics enables a superior electrolyte microstructure and high PCEC performance.

dense microstructure↗
DOE OSTI2017

Cold sintering process of Li 1.5 Al 0.5 Ge 1.5 (PO 4 ) 3 solid electrolyte

Abstract The recently developed technique of cold sintering process (CSP) enables densification of ceramics at low temperatures, i.e., <300°C. CSP employs a transient aqueous solvent to enable liquid phase‐assisted densification through mediating the dissolution‐precipitation process under a uniaxial applied pressure. Using CSP in this study, 80% dense Li 1.5 Al 0.5 Ge 1.5 (PO 4 ) 3 (LAGP) electrolytes were obtained at 120°C in 20 minutes. After a 5 minute belt furnace treatment at 650°C, 50°C above the crystallization onset, Li‐ion conductivity was 5.4 × 10 −5 S/cm at 25°C. Another route to high ionic conductivities ~10 −4 S/cm at 25°C is through a composite LAGP ‐ (PVDF‐HFP) co‐sintered system that was soaked in a liquid electrolyte. After soaking 95, 90, 80, 70, and 60 vol% LAGP in 1 M LiPF 6 EC‐DMC (50:50 vol%) at 25°C, Li‐ion conductivities were 1.0 × 10 −4 S/cm at 25°C with 5 to 10 wt% liquid electrolyte. This paper focuses on the microstructural development and impedance contributions within solid electrolytes processed by (i) Crystallization of bulk glasses, (ii) CSP of ceramics, and (iii) CSP of ceramic‐polymer composites. CSP may offer a new route to enable multilayer battery technology by avoiding the detrimental effects of high temperature heat treatments.

Berbano, Seth S.↗
DOE OSTI2019

Dielectric and piezoelectric properties of 0.970(0.95(K{sub 0.485}Na{sub 0.515})NbO{sub 3}–0.05LiSbO{sub 3})–0.015CuO–0.015Al{sub 2}O{sub 3}/PVDF 0–3 composite reinforced with two kinds of ZnO powder

0.970(0.95(K{sub 0.485}Na{sub 0.515})NbO{sub 3}–0.05LiSbO{sub 3})–0.015CuO–0.015Al{sub 2}O{sub 3} (KNNLS–CA) ceramic powder obtained through the conventional solid state reaction. The ZnO nanoparticles (denoted as ZnO1) and poly (vinylidene fluoride) (PVDF) were supplied from commercial companies. The self-synthesized ZnO powder (denoted as ZnO2) were prepared by hydrothermal method using Zn (CH{sub 3}COO){sub 2}·2H{sub 2}O and NaOH. Subsequently, the two kinds of composites were fabricated by hot-pressing process using KNNLS–CA ceramic powder, two kinds of ZnO powder and PVDF polymer. The effects of the ZnO on the crystalline structures, morphology, thermal stability, densities and electric properties of composites were studied systemically. The KNNLS–CA ceramic possesses a perovskite phase with orthorhombic symmetry and peaks from the second phase of K{sub 3}Li{sub 2}Nb{sub 5}O{sub 15} (PDF#52-0157) are detected by X-ray diffraction. PVDF polymer mainly possesses α, β and γ phases. Two kinds of ZnO all possess hexagonal wurtzite structures without any impurity phase. It is worth noting that the ZnO particles have great impacts on lattice constants, strain and crystallinity. In addition, the ZnO particles can enhance the relative fraction of β phase in PVDF and improve the thermal stability of the composite. Interestingly, the dielectric and piezoelectric properties are also found to be improved with the increase of ZnO content. Especially, when 10 wt.% ZnO2 is doped, the dielectric permittivity reaches the value of 586.4 (100 Hz) at room temperature and the piezoelectric constant is 64 pC/N. After 30 days of aging test, it is obvious that all the composites present a good stability of piezoelectric property.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Processing and consolidation of copper/tungsten

Here, we developed a copper/tungsten (Cu/W) composite for mesoscale Materials Science applications using the novel High-Energy Diffraction Microscopy (HEDM) technique. Argon-atomized copper powder was selected as the starting raw powder and screened to remove the extremely large particle fraction. Tungsten particles were collected by milling and screening the -325 mesh tungsten powder between 500 and 635 mesh sieves. Hot pressing of screened Cu powder was performed at 900 °C in Ar/4 %H 2 atmosphere. XRD and ICP results show that the hot-pressed Cu sample consists of about 5 vol% Cu 2 O, which is caused by the presence of oxygen on the surface of the starting Cu powder. Hot pressing the copper powder in a pure hydrogen atmosphere was successful in removing most of the surface oxygen. Our process was also implemented for hot pressing the Cu/W composite. The density of the Cu/W composites hot pressed at 950 °C in pure hydrogen was about 94 % of the theoretical density (TD). The hot-pressed Cu/W composites were further hot isostatic pressed at 1050 °C in argon atmosphere, which results in 99.6 % of the TD with the designed Cu grain size and W particle distribution. Tensile specimens with D-notch were machined using the wire EDM method. Furthermore, the processing and consolidation of these materials will be discussed in detail. The HEDM images are also showed and discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Progress and Technology Assessment of Melt-Cast Ceramic Waste Forms

The Savannah River National Laboratory (SRNL) conducted research from FY2011 – FY2020 to develop ceramic waste forms to treat High-Level Waste (HLW) resulting from reprocessing of commercial Used Nuclear Fuel (UNF) as part of the Department of Energy (DOE) office of Nuclear Energy (NE) Fuel Cycle Technologies (FCT) research program. The objective of the research was to develop a reference ceramic waste form and process technology needed to immobilize the combined HLW raffinate stream, including undissolved solids and soluble technetium, and potentially the TRU waste stream resulting from reprocessing processes. This report compiles the relevant literature produced under, and pertinent to, the program objectives and provides a perspective on the technology development as well as prospects for future.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

X-ray characterization technique for the assessment of surface damage in GaN wafers

SixPoint Materials has successfully switched to production of two-inch diameter GaN wafers using the ammonothermal method. Crystal quality values are high with dislocation densities typically in the low 10 5 cm -2 . In efforts to produce true epi-ready material, investigations were made to develop a technique to study surface damage caused by the back-end process using X-ray diffraction methods. Analysis of peak tailing from X-ray rocking curves of the (1 1 4) reflection indicates the progression of surface damage during each step of the back-end process. For instance, the tailing can be partially represented using full width five thousand max (FW5000M) values. By using a peak with a low glancing angle, such as the (1 1 4) reflection’s angle of 10.8662°, more of the X-ray beam is scattered in the surface region, providing an improved measurement of surface damage. Since this technique is non-destructive and can be performed without dismounting the sample from its ceramic back-end processing plate, it can provide information on the damaged layer at each stage of the back-end process. Using this technique to evaluate samples from various manufacturers, we found a lack of uniformity in surface damage from GaN companies. It is our hope that this technique will be adopted to better standardize surface damage measurements in the GaN field.

36 MATERIALS SCIENCE↗
DOE OSTI2019

A Python Package for Fuel Cycle and Waste Management Analysis - 19545

The future of nuclear power utilization in the United States may involve a transition from the once-through light water reactor fuel cycle to a so-called advanced fuel cycle. An advanced fuel cycle may offer improvements in natural resource utilization, reactor safety, and environmental impact. In addition, adoption of an advanced fuel cycle will result in changes in the amount, composition, and disposal of the nuclear wastes they produce. Characteristics intrinsic to the wastes themselves, such as mass and radioactivity at specific times, were used as waste management metrics in the Department of Energy 2014 Fuel Cycle Evaluation and Screening (FCES) study. Binning of these metrics informed fuel cycle according to relative potential benefit. However, waste properties alone cannot qualify management strategy. Therefore, comparing fuel cycles from the perspective of waste management can provide additional insights. To that end, an object-oriented Python package has been developed to perform fuel cycle waste management calculations. The package, named nwpy (short for Nuclear Waste analysis in Python), mimics the mass flow operations reported in the FCES study and interfaces with the ORIGEN-S code to assess metric data as reported in the FCES. In addition, this Python package determines the loading of waste streams into forms suitable for final disposal in a geological repository and uses such data for repository performance assessment. This work describes the Python package methodology, assumptions, and capabilities. As input data, the package requires information about the fuel cycle such as the mass of fuel discharged, the cooling time between reactor discharge and subsequent operations, and the separations process efficiencies and waste forms it produces. In addition, the isotopic composition of the reactor discharge stream, such as that available from the FCES database, is required. With that, it can perform prescribed mass flow and decay operations throughout the back end of the fuel cycle, the latter carried out by the ORIGEN-S code distributed with the SCALE6.2 software suite. The result is time-dependent data characterizing the waste on a per-package basis. Package loading for waste streams depends on the stream form (i.e. UNF vs. HLW, or glass HLW from aqueous reprocessing vs. ceramic HLW from electrochemical processing) and is based on literature review and engineering assumption. As an example of the application of the code, calculations for the areal footprint of direct-contact repositories for different fuel cycles is shown. Development is ongoing, and the package is expected to grow incorporating capabilities for waste management analyses such as waste transportation and radionuclide transport through the biosphere. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗